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HCID 66839446, 화합물 → HCID 66839152, 화합물

HRID 546746
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HRID 546746 반응식
[CH3:1][O:2][C:3]1[N:8]=[C:7](/[CH:9]=[C:10](\[CH3:18])/[C:11]([O:13]C(C)(C)C)=[O:12])[CH:6]=[CH:5][C:4]=1[N:19]1[CH:23]=[C:22]([CH3:24])[N:21]=[CH:20]1>FC(F)(F)C(O)=O.C(Cl)Cl>[CH3:1][O:2][C:3]1[N:8]=[C:7](/[CH:9]=[C:10](\[CH3:18])/[C:11]([OH:13])=[O:12])[CH:6]=[CH:5][C:4]=1[N:19]1[CH:23]=[C:22]([CH3:24])[N:21]=[CH:20]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 66839446HCID 66839446, 화합물

생성물 1

HCID 66839152HCID 66839152, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

A mixture of 6-chloro-2-methoxy-3-(4-methyl-1H-imidazol-1-yl)pyridine (400 mg), an allylpalladium chloride dimer (32.8 mg), tri-o-tolylphosphine (54.4 mg), sodium acetate (441 mg), dimethylacetamide (0.640 mL), tert-butyl methacrylate (0.724 mL) and toluene (2 mL) was stirred in a nitrogen atmosphere at 120° C. for 3.5 hours. The reaction solution was left to cool to room temperature. Then, a silica gel was added and the reaction solution was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system) to obtain 313 mg of tert-butyl (E)-3-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]-2-methylacrylate. The ester was diluted with trifluoroacetic acid (2.48 mL) and methylene chloride (2.48 mL), and the reaction solution was stirred at room temperature for 3.5 hours. The reaction solution was concentrated under reduced pressure to obtain 260 mg of the title compound. The property value of the compound is as follows.

후처리

  1. concentrationThe reaction solution was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-2b7f47c86d27487cb447b1340531e7c3
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07935815B2

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